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Journal of Agriculture and Livestock Farming

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Original Article
A study on approaches to uncertainty assessment in XRD analysis for determining inorganic compounds in complex waste materials
Daniela Rizzo1, Debora Cusumano1, Laura Borgese2, Annalisa Zacco2, Eleonora Cuccia3, Silvia Maltese4 and Marco Volante4  
D.RIZZO@arpalombardia.it
1U.O. Laboratorio Regionale Area Est – Dipartimento Prestazioni Analitiche – ARPA Lombardia, Via Cantore 20, 25128 Brescia, Italy
2Dipartimento di Ingegneria Meccanica ed Industriale, DIMI - Università di Brescia - Via Branze 38, 25123 Brescia, Italy
3U.O. Qualità dell’Aria - Direzione Generale – ARPA Lombardia, Via Rosellini 17, 20124 Milano, Italy
4U.O. Accreditamento e Sviluppo Tecnico Scientifico - Dipartimento Prestazioni Analitiche – ARPA Lombardia, Via Rosellini 17, 20124 Milano, Italy
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ABSTRACT

A study was done to estimate the uncertainty of waste analysis by XRD technique on powder samples. The XRD technique is important for identifying crystalline phases and inorganic compounds to give information about hazardousness on unknown wastes. No reference materials or proficiency tests are available for these sometimes very complex and heterogeneous matrices. The present study was done on a real sample with a metrological approach. The matrix complexity in the considered sample, even after grinding, is increased by the fact that there is a fibrous fraction and a nonfibrous powdery fraction mixed together. Accuracy was checked by analysis with other techniques and at other laboratories. The results showed that external calibration with single pure standard is prone to large errors compared with the use of multi-level external calibration. The approach that best accounts for matrix complexities is however the method of standard additions. The level of uncertainty determined was within ±50% as the expanded uncertainty (k~2, conf. level 95%).



KEYWORDS

    1. Wastes
    2. X-Ray diraction
    3. Uncertainty


Author Info

Daniela Rizzo1, Debora Cusumano1, Laura Borgese2, Annalisa Zacco2, Eleonora Cuccia3, Silvia Maltese4 and Marco Volante4

1U.O. Laboratorio Regionale Area Est – Dipartimento Prestazioni Analitiche – ARPA Lombardia, Via Cantore 20, 25128 Brescia, Italy
2Dipartimento di Ingegneria Meccanica ed Industriale, DIMI - Università di Brescia - Via Branze 38, 25123 Brescia, Italy
3U.O. Qualità dell’Aria - Direzione Generale – ARPA Lombardia, Via Rosellini 17, 20124 Milano, Italy
4U.O. Accreditamento e Sviluppo Tecnico Scientifico - Dipartimento Prestazioni Analitiche – ARPA Lombardia, Via Rosellini 17, 20124 Milano, Italy
Corresponding author: D.RIZZO@arpalombardia.it

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